Formic acid extractions of Brazil nut and babassu coconut samples were undertaken prior to determination of Al, As, Ba, Co, Cr, Cu, Mn, Mo, Ni, Pb, Se, Sr, V and Zn in their meat and oil portions by inductively coupled plasma mass spectrometry (ICP-MS) in an effort to accomplish a first order fractionation of the trace elements between these two components. An optimized full factorial design was applied to establish the best conditions for extraction. Microwave-assisted nitric acid digestions of samples and fractions along with analysis of certified reference material TORT-2 established the efficiency of recovery of the trace elements as well as provided a verification of accuracy. The multiple responses were analyzed using a desirability function wherein the recovery of the trace elements by extraction was compared with the determination of the total content as determined by nitric acid digestion. Although most trace elements presented a recovery higher than 85% using a formic acid extraction, Al suffered consistently low results for all samples (40-50%). Except for Al and Cr, the majority of the trace elements were present in the defatted fraction of both samples, i.e., Al (50 and 10%), Cr (86 and 60%), Ni (30 and 10%) and Sr (8 and 20%) in Brazil nut and babassu coconut oil fractions, respectively.